Abstract: A ternary complex of Zr(Ⅳ )-EDTA-Stilbazo has been investigated and found to be a highly selective system for the spectrophotometric determination of Zr(Ⅳ). Zirconium (Ⅳ) forms an orange-red coloured ternary complex with Stilbazo and EDTA at pH 5.6-6.6. The complex exhibits maximum absorption at 503nm, where the apparent molar absorptivity is 2.8×10⁴. The molar ratio of the three components in the complex is estimated to be Zr(Ⅳ) :EDTA : Stilbazo = 1: 1: 1 by the Job's method and molar ratio method. Beer's law is obeyed in the range of 0-50μg Zr/25ml.A highly selective method has been developed for the rapid determination of micro amounts of zirconium in nickel-base alloy and Al-Mg alloy without separating Zr from the accompanying elements.The results are satisfactory.